Fixation of nitrogen by means of titanium and its transformation into industrial products



Patented. Mar. 18, 1924.

easi- PAUL ANDREU AND RENE PAQUET, 0F PARIS, FRANCE.

FIXATION or NITROGEN BY MEANS or TITANIUMVAND ITs TRANSFORMATION INTo INDUSTRIAL PaonU'oTs.

No Drawing.

To all whom, it may concern:

Be it known that we, PAUL ANDREU and RENE Pxonnr, citizens of the French Republic, residing at Paris, Department of the Seine, in France, have invented certain new and useful Improvements in the Fixation of Nitrogen by Means of Titanium and Its Transformation into Industrial Products, of which the following is a specification.

The present invention has for its object the fixation of nitrogen by means of titanium and its transformation into industrial products, such as cya-nides, ammonia, etc., together with, if desired, the extraction of the titanium contained in minerals such as titanium irons, rutiles, anatase, etc.

If the extraction of the titanium or its salt-s be desired, the following process is employed:

The titanium ore is mixed with charcoal and a salt of a metal, alkali, alkaline earth or the like (for example sodium carbonate). The whole is then reduced to powder. The quantities to beused are varied in accor ance with the analysis of. the ore. The following|mixture is given by way of example:

Kgs.

Titanium iron ore containing 40% Tio 1,000 Sodium carbonate 7 50 Charcoal 1,000

This mixture should be heated in an atmosphere of nitrogen to atemperature not exceeding 1,850 C. The mixture will absorb the nitrogen and will give nitrides and carbides, etc., which will then be subjected to the action of steam at a temperature not exceeding 1.800 6., giving off ammonia,hydrocyanic acid, etc. These various products will be collected by means of suitable washing or condensing apparatus.

The mass, havingbeen subjected to the action f steam will contain a large part of the metals in the form'of oxides and the titanium in the form of titanate which can be extracted by washing with water, acids, and bases. The washing with water dissolves the titanate and thereby separates the titanium from the iron. The titanium solution is then precipitated by hydrolysis by the action of acids or bases.

After washing, filtering, drying and calcining at a. high temperature an anhydrous Application filed January 13, 1922. Serial No. 529,028.

product composed of titanium oxide will be obtained.

The above description is given by way of example only and the details can be modified without departing from the scope of the invention, which consists in fixing the nitrogen in the presence of or by means of tita nium and forming therefrom industrial products with the possibility of separating the titanium or its salts. It will be understood the fixation of the nitrogen only may be effected by employing modifications of the above process such, for instance, as nitrogenizing a mixture of the ore and charcoal only, then subjecting it to the action of steam and recovering the volatile products (in which case the solid residue can be employed over again) lixiviation may follow the nitrogenizing thus obtaining directly cyanides, sulpho-cyanides, terro-cyanides, etc.

1. A process of producing titanium oxid with simultaneous recovery of nitrogen compounds which comprises mixing a titanium containing ore, with about. an equa weight of carbonaceous material and amount of an alkali corresponding to about three-fourths said weight of sodium carbonate, subjecting the mixture to an atmosphere containing free nitrogen at a temperature near 1850 0., and thereafter subjecting the resulting product to action of steam at near 1800 C., whereby nitrogen compounds are evolved. leaching the solid product with water whereby the soluble titanium compounds are separated from iron and other insoluble materials, subjecting the resulting solution to hydrolytic dissociation and calcining the product.

2. A process of producing titanium oxid with simultaneous recovery of nitrogen compounds which comprises mixing one hundred parts of titanium ore containing about 40% TiO one hundred parts of carbon and seventy-five parts of Na CQ subjecting the mixture to an atmosphere containing free nitrogen at a temperature near 1850 C-., and thereafter subjecting the resulting product to action of steam at near 1800 C. whereby nitrogen compoundsare evolved, leaching the solid product with water whereby the soluble titanium compounds are separated from iron and other insoluble materials, subjecting the result' ing solution to hydrolytic dissociation and sponding to about 75 parts by wei ht of calcining the product. sodium carbonate to each 40 parts 0t TiO.

3. A process which comprises heating to n h saifi v 10 a hi h temperature, i an atmosphere f 1n test1mony whereof we hereunto aflix 5 nitrogen, a mixture containing titanium our slgnatul'esore, alkali and a carbonaceous material, the PAUL ANDREI]- proportion of alkali to titanium ore corre- RENE PAQUET. 

